UNIT3 PRACTICAL

Reference section SKILLS

A — Inorganic compounds and elements

1 Appearance

• Coloured crystalline substances are usually hydrated salts of transition metals.

The colour of the solid substance may provide evidence for its identity.

Colour Possible transition metal ions in salt

blue copper(II)
pale green iron(II)
green copper(II), chromium(III), nickel(II)
purple manganate(VII)
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brown iron(III)
pink manganese(II)
yellow chromate(VI)
orange dichromate(VI)

• The colours of transition metal ions in dilute, aqueous solution are shown in the table
below.

Colour Possible identity

blue copper(II)
green iron(II), chromium(III), nickel(II)
brown / yellow iron(III)
pale pink manganese(II)
yellow chromate(VI)
orange dichromate(VI)
purple manganate(VII)
colourless zinc(II)

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 2 Flame tests

• To carry out a flame test, a clean nichrome wire is used to mix a sample of a solid with
one drop of concentrated hydrochloric acid. The wire is held in progressively hotter
parts of a non-luminous Bunsen flame.

Flame colour Inference

yellow sodium ion
lilac potassium ion
yellow-red* calcium ion
red* lithium or strontium ion
pale green barium ion

* Further tests would be needed to distinguish these ions.

3 Heating
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• Gases or vapours may be evolved on heating a solid compound.

Gas or vapour Possible source

carbon dioxide carbonates of metals other than group 1
oxygen group 1 nitrates (other than Li)
oxygen and nitrogen nitrates (other than Na or K)
dioxide
water hydrated salts

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 4 Recognition and identification of common gases

Gas Observations
oxygen colourless gas which relights a glowing splint
carbon dioxide colourless gas which gives a white precipitate with
limewater (calcium hydroxide solution)
ammonia colourless gas which turns moist red litmus paper blue and
forms white smoke with hydrogen chloride
nitrogen dioxide brown gas*
hydrogen colourless gas which ignites with a ‘pop’
hydrogen chloride steamy fumes on exposure to moist air, acidic and forms
white smoke with ammonia
chlorine pale green gas which bleaches moist litmus paper
bromine brown gas*
iodine purple vapour
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water vapour turns blue cobalt chloride paper pink

* Bromine dissolves in organic solvents to form a brown solution whereas nitrogen

dioxide is insoluble.

5 Action of dilute acids

• When dilute sulfuric or hydrochloric acid is added to a substance a gas may be evolved
or there may be a colour change in the solution.

Action of acid Possible source

carbon dioxide evolved carbonate
hydrogen evolved a metal
yellow solution turns orange chromate(VI) to dichromate(VI)
sulfur dioxide evolved and pale yellow thiosulfate
precipitate formed

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 6 Tests for oxidizing and reducing agents

Reducing agents usually:

decolourise aqueous acidified potassium manganate(VII) and
may also turn aqueous, acidified potassium dichromate(VI) from orange to green.
Reducing agents include:
iron(II) ions
iodide ions
hydrogen peroxide.

Oxidizing agents usually:

liberate iodine as a brown solution or black solid from aqueous potassium iodide.
Iodine solution gives a blue-black coloration with starch.
Oxidizing agents include:
acidified manganate(VII) ions
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acidified dichromate(VI) ions
hydrogen peroxide
copper(II)ions
aqueous chlorine
aqueous bromine.

7 Hydrogen peroxide solution

Aqueous hydrogen peroxide (H2O2) can act as both an oxidizing and a reducing agent often
with the evolution of oxygen, although this may be unreliable.

Observation on adding H2O2 Inference

brown precipitate manganate(VII), brown precipitate is
MnO2
purple solution is decolourised manganate(VII) in acid solution

pale green solution turns yellow iron(II) to iron(III) in acid solution

green precipitate turns brown iron(II) hydroxide to iron(III) hydroxide

green alkaline solution goes yellow chromium(III) to chromate(VI)

brown solution or black precipitate iodine from iodide in acid solution

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 B — Precipitates

When two aqueous solutions are mixed together and an insoluble compound is formed this is
known as a precipitate not a suspension. The observation that a precipitate is formed should
always be accompanied by the colour of the precipitate, even if this is white. Some reagents
should be added until they are in excess. This may result in a precipitate forming then
dissolving in excess reagent.

1 Sodium hydroxide solution

• When dilute sodium hydroxide (NaOH) solution is added to a solution containing a

metal ion a precipitate of the insoluble hydroxide, eg Mn(OH)2, is usually formed.
Precipitates which are amphoteric hydroxides will dissolve in excess sodium hydroxide
to give a solution containing a complex ion, eg [Cr(OH)6]3−.
• Students should assume that aqueous sodium hydroxide should be added until it is in
excess even if this is not explicitly stated in the instructions.
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Observation on adding dilute Observation on adding Likely ion
NaOH excess dilute NaOH
green precipitate precipitate dissolves to a chromium(III)
green solution
off-white precipitate which precipitate is insoluble manganese(II)
darkens on exposure to air
green precipitate which turns precipitate is insoluble iron(II)
brown on exposure to air
brown precipitate precipitate is insoluble iron(III)

green precipitate precipitate is insoluble nickel(II)

blue precipitate precipitate is insoluble copper(II)

white precipitate precipitate dissolves to a zinc(II)

colourless solution
white precipitate precipitate is insoluble magnesium, barium,
strontium, calcium
no precipitate sodium, potassium

no precipitate but ammonia ammonium

evolved on warming

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 2 Ammonia solution

• Dilute aqueous ammonia (NH3), when added to a solution containing a cation, will form
the same hydroxide precipitate as dilute sodium hydroxide solution, eg Mn(OH)2. Excess
aqueous ammonia may dissolve the precipitate to form a complex ion, eg
[Cu(NH3)4(H2O)2]2+.
• Students should assume that aqueous ammonia must be added until it is in excess.

Observation on adding dilute Observation on adding excess Likely ion

aqueous NH3 dilute aqueous NH3
green precipitate precipitate is soluble to give chromium(III)
green solution
off-white precipitate precipitate is insoluble manganese(II)
green precipitate turning precipitate insoluble iron(II)
brown
brown precipitate precipitate insoluble iron(III)
green precipitate precipitate dissolves to give nickel(II)
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blue solution
blue precipitate precipitate dissolves to give copper(II)
deep blue solution
white precipitate precipitate dissolves to give zinc(II)
colourless solution
white precipitate precipitate is insoluble magnesium

3 Barium chloride solution

• Aqueous barium chloride forms precipitates of insoluble barium salts with a number of
anions but is usually used as the test for the sulfate, SO42−, ion. Aqueous barium
chloride is usually used with dilute hydrochloric acid.

Anion Precipitate Addition of dilute HCl

colour formula
sulfate white BaSO4 precipitate is insoluble
sulfite white BaSO3 precipitate dissolves
carbonate white BaCO3 precipitate dissolves with effervescence

If dilute hydrochloric acid is added to the anion solution before aqueous barium chloride
then only the sulfate will form as a precipitate.

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 4 Silver nitrate solution

• Aqueous silver nitrate is commonly used to test for the presence of halide ions in
solution. Anions which would interfere with the test (eg carbonate) are removed by
adding dilute nitric acid before the aqueous silver nitrate.
• The identity of a halide may be confirmed by the addition of aqueous ammonia, (NH3),
both dilute and concentrated.
• Silver halides which dissolve in ammonia do so to form a colourless solution of the
complex ion, [Ag(NH3)2]+.

Anion Precipitate Addition of aqueous NH3

colour formula dilute concentrated
chloride white AgCl soluble
bromide cream AgBr soluble in excess soluble
iodide yellow AgI insoluble insoluble
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5 Concentrated sulfuric acid

• When a few drops of concentrated sulfuric acid (H2SO4) are added to a solid halide the
observed reaction products may be used to identify the particular halide ion present.
This is a potentially hazardous reaction.
• It must be carried out on a small scale and in a fume cupboard.
• The products in brackets will not be observed since they are colourless gases. The
halide ion may be identified without the need to test for these gases. No attempt
should ever be made to detect these gases by smell.

Halide Observations on adding Observed reaction

concentrated H2SO4 products
chloride steamy fumes, vigorous reaction HCl

bromide steamy fumes, brown vapour, HBr, Br2 (SO2)

vigorous reaction
iodide steamy fumes, black solid, purple HI, I2, S, (H2S)
vapour, yellow solid, vigorous
reaction

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 C — Organic compounds

Students will always be told if a compound, or mixture of compounds, to be identified is

organic. Often the molecular formula, or the number of carbon atoms in a molecule, of a
compound will be given. Chemical tests may be followed by spectroscopic information.

1 Appearance

Simple organic compounds are usually colourless liquids or white solids. It is unlikely that
appearance alone will provide firm evidence for identification.

2 Solubility

Solubility of compound Possible identity pH of Possible

solution identity
dissolve in water simple alcohols, simple above 7 amines
carboxylic acids,
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propanone, simple
aldehydes, simple below 7 carboxylic
amines and their salts acids,
phenols
dissolve in dilute acid amines
but may not dissolve in
water
dissolve in aqueous carboxylic acids, phenols
alkali but may not
dissolve in water

3 Ignition

Igniting an organic unknown on a crucible lid may help in identifying it.

Observation Possible inferences

burns with a smoky flame aromatic, unsaturated eg alkene

burns with a clean flame saturated low molar mass compound

no residue most lower molar mass compounds

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 4 Chemical tests

The details of how these tests are to be carried out will be included in the instructions to
students in the assessment activities.

Test Observation Inference

warm with acidified potassium orange to green primary or secondary
dichromate(VI) solution alcohol, aldehyde
yellow solution is alkene
decolorised
shake with bromine water
if white phenol
precipitate also
formed
warm with aqueous precipitate: halogenoalkanes:
sodium/potassium hydroxide, acidify
white C−Cl
with dilute nitric acid then add
aqueous silver nitrate cream C−Br
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yellow C−I

phosphorus(V) chloride steamy fumes of OH group in alcohols

HCl that turn damp and carboxylic acids
blue litmus paper
red

2,4−dinitrophenylhydrazine solution orange precipitate C=O group in

aldehydes and
ketones

boil with Fehling’s or Benedict’s blue solution gives aldehyde

solution red precipitate

warm with ammoniacal silver nitrate silver mirror aldehyde

(Tollens’ reagent)

sodium or potassium carbonate or effervescence carboxylic acid

hydrogencarbonate solution

add a small piece of sodium effervescence alcohol, phenol or

(bubbles), sodium carboxylic acid
dissolves, white
solid formed
warm with carboxylic acid and a few ester smell, eg alcohol
drops of concentrated sulfuric acid glue-like

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 Test Observation Inference
sodium nitrite and dilute hydrochloric orange precipitate aromatic amine
acid followed by an alkaline solution
of phenol in ice-cold conditions

iodine in alkaline solution pale yellow methyl ketone or

precipitate ethanal,
C CH3
O
methyl secondary
alcohol or ethanol
CH CH3
OH
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 D — Spectroscopy

Modern instrumentation plays a vital role in the characterisation and identification of

molecules and ions. The sections which follow will enable interpretation of the data likely to
be presented to students.

1 Mass spectrometry

Simplified mass spectra will be given which may be interpreted in two main ways.
1 The value of the compound’s relative molar mass may be obtained from the m/e value of
M+, the molecular ion. This will have the highest value of m/e. This need not necessarily
be the ‘base’ peak, which is simply the most abundant ion. Questions will be set in such a
way that students will not be confused by the presence of a line due to the (M + 1) ion.
2 The fragmentation pattern of the spectrum gives useful information about the structure of
the molecule. For example, a peak at m/e 29 is likely to be due to the presence of a C2H5
group in the molecule. Students are reminded that, when asked, they should give
displayed structures for fragments, which must carry a positive charge also.
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2 Infrared spectroscopy

This is a very powerful non-destructive technique which provides information regarding the
nature of covalent bonds within the molecule.
Students should look at the most intense absorptions to quickly gain structural clues. Table 1
provides sufficient details to enable the principal bands to be assigned. Students should
remember that absorption frequency is affected by the chemical environment and that
absorption may take place outside the range given.
The connection between structures should be recognised. For instance, an alcohol [O-H]
stretch will be accompanied by a [C-O] stretch.
Please see the Data booklet for specific IR spectroscopy data.

3 Nuclear magnetic resonance (nmr)

Nuclear magnetic resonance spectra may be included as part of an investigation into

structure. Spectra will be high resolution with possible spin–spin coupling displayed.
Please see the Data booklet for specific nmr data.

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